Bi_(3.15)Nd_(0.85)Ti_3O_(12)纳米管阵列的制备与微结构表征

采用溶胶凝胶法,在孔径为200 nm的阳极氧化铝模板中制备了Bi_3.15Nd_0.85Ti_3O_(12)纳米管阵列.通过XRD、SEM、TEM、HRTEM、SAED和Raman光谱测试手段对纳米管阵列的物相、微结构和声子振动特性进行了表征.研究表明,所合成BNdT纳米管为钙钛矿相多晶结构,纳米管外径约为200 nm,管壁厚约10 nm,管径和长度与所用AAO模板尺寸一致.Raman光谱分析表明,Nd离子取代了类钙钛矿层中A位的Bi离子.     

锆钛酸铅纳米管制备工艺研究

研究了溶胶-凝胶浸渍阳极氧化三氧化二铝（AAO）模板法制备Pb(Zr0.52Ti0.48)O3（PZT）一维纳米结构的工艺方法。试验结果表明,以硝酸氧锆、醋酸铅、钛酸丁酯（按0.52:1:0.48的摩尔配比）为原料,以乙二醇为溶剂,可获得稳定的PZT溶胶,通过反复滴加浸渍氧化铝模板,最终经650 ℃晶化处理和腐蚀AAO后得到PZT纳米管。样品表征结果说明,制得的PZT纳米管为钙钛矿相,表面结构完整、孔径均一、排列均匀整齐,长50 μm、管径300 nm、壁厚40 nm。     

溶胶凝胶模板法合成ITO纳米管及其氢敏性能

采用简单的溶胶凝胶阳极氧化铝模板法制备了ITO纳米管.通过FE-SEM、HRTEM、XRD对其微观形貌、结构、相组成等进行了表征和分析,并测试了其对H_2的气敏特性.结果表明,所得纳米管是由10～20 nm晶粒组成的多晶结构,壁厚约为25 nm,平均直径约250 nm,与AAO (Anodic Aluminum Oxide)模板的直径相同.产物在550 ℃热处理后为立方铁锰矿结构的In_2O_3,Sn~(4+)已经掺杂到In_2O_3的晶格中.所得ITO纳米管常温下对氢气具有较好的敏感性及稳定性.     

溶胶一凝胶模板法制备氧化镍纳米线

采用二次阳极氧化的方法,以5%磷酸为电解液,制得具有一定厚度有序性较高的阳极氧化铝模板(AAO),结合溶胶-凝胶法在模板微孔内合成氧化镍纳米线.利用扫描电镜(SEM)对模板和纳米线材料的形貌进行了表征,结果表明:采用该方法成功制得线状的氧化镍,长度可达亚微米级,直径约为100nm,与AAO模板的孔径大小基本一致,因此可以通过调节AAO模板的孔径大小来实现氧化镍纳米线的可控生长.     

原位模板法在铝基底上制备TiO2纳米管阵列薄膜

采用液相沉积法，将铝基多孔阳极氧化铝（AAO）模板浸入到（NH4）2TiF6溶液中，制备出高度有序的TiO2纳米管阵列薄膜，并在不同的温度下进行了热处理。用场发射扫描电子显微镜、透射电子显微镜和X射线衍射仪等手段对试样的微观形貌、结构及物相进行了表征。结果表明，TiO2纳米管的形貌依赖于AAO的特征，薄膜是由外径大约200nm，壁厚约40nm的TiO2纳米管阵列组成，薄膜厚度约25μm。原位模板法制备的TiO2纳米管阵列薄膜为非晶态，在400℃空气中焙烧2h转变为锐钛矿相TiO2。经过650℃焙烧仍保持纳米管结构，表现出较好的热稳定性。     

玻璃先驱体对溶胶-凝胶合成纳米氧化铝的影响

以硝酸铝、硝酸镁、硝酸钙、硅溶胶为原料,采用溶胶-凝胶法合成纳米级氧化铝粉体,并对不同温度煅烧后粉体的物相与形貌进行表征。通过在硝酸铝的溶胶中引入4%(质量分数)的MgO-CaO-Al2O3-SiO2玻璃助剂先驱体,在80℃水浴中长时间静置后获得乳白色凝胶,在不同温度下煅烧该凝胶,结果发现:煅烧温度低于950℃时,所获得的粉体主要为无定型态,仅含有少量的γ型氧化铝;将凝胶在1000℃煅烧2h后,全部变成粒度在25～35nm、粉体颗粒呈球形的α型氧化铝;玻璃助剂先驱体的添加,不但降低了α-Al2O3的合成温度,同时还加快了γ-Al2O3向α-Al2O3的转变进程。     

两步沉淀法合成Bi3.25La0.75Ti3O12(BLT)粉体及其表征

以五水硝酸铋(Bi(NO3)3·5H2O)、水合硝酸镧(La(NO3)3·nH2O)和钛酸四丁酯((C4H9O)4Ti)为原料,氨水为沉淀剂,分两步沉淀Ti离子和Bi、La离子,利用沉淀法合成了Bi3.25La0.75Ti3O12(BLT)粉体.利用差热分析(DTA)和热失重(TG)对两步沉淀法制备的前驱体粉体的热行为进行了分析,用X射线衍射(XRD)研究了其晶相演化过程,利用场发射扫描电子显微镜(FESEM)对BLT粉体粒度和形貌进行了观察.结果显示两步法制备的前驱体粉体经低温煅烧直接转化为单一的铋层状钙钛矿相BLT粉体,在700℃煅烧2 h合成的BLT粉体颗粒不大于100nm,颗粒间结合疏松,具有良好的分散性.     

利用PS模板制备多孔SrFe12O19薄膜的研究

本文以提拉浸渍法使用聚苯乙烯(PS)球模板制备了有序多孔结构的锶铁氧体(SrFe12O19)薄膜。将微乳液聚合法合成的PS球,通过提拉浸渍法有序地组装在硅片基板上形成PS模板;使用溶胶-凝胶法制备SrFe12O19前驱体溶胶,再采用提拉浸渍法使SrFe12O19前驱体溶胶填充PS模板的空隙,在900 ℃保温2 h去除PS球后即制得多孔SrFe12O19薄膜。重点研究了聚乙烯吡咯烷酮(PVP)的含量对PS球微观形貌,浸渍时间对PS模板以及多孔SrFe12O19薄膜微观形貌的影响,并对多孔SrFe12O19薄膜的形成机理进行了讨论,建立了相应的模型。结果表明：添加0.2 g的PVP可得到粒径均匀的PS球,且微球之间空隙明显;将硅片在PS球乳液中浸渍10 s可得到单层有序的PS模板;当PS模板在SrFe12O19前驱体溶胶中浸渍10 s时可制备出孔径约200 nm的蜂窝状多孔结构的纯SrFe12O19相薄膜,其表现出优异的硬磁性能：饱和磁化强度为27.9 emu/g,剩磁为15.5 emu/g,矫顽力为2613.4 Oe。     

氧化钕纳米线的制备与表征

以硝酸钕和尿素为主要原料,多孔阳极氧化铝膜(AAO)为模板,分别采用普通浸渗和压力浸渗法制备了氧化钕纳米线.采用扫描电子显微镜(SEM)、透射电子显微镜(TEM),X射线衍射仪(XRD)和能量仪(EDS)对纳米线的形貌,结构及组成进行了表征.结果表明:两种浸渗方法均可得到氧化钕纳米线,压力溶胶浸渗有利于模板纳米孔填充度的提高,可以得到高长径比的氧化钕纳米线.     

水热法氧化钒纳米管生长过程的研究

以十二胺和五氧化二钒为原料通过水热反应合成了氧化钒纳米管，并用X射线衍射仪(XRD)和高分辨透射电子显微镜(HRTEM)进行表征。实验结果表明，用这种方法合成的氧化钒纳米管转化率很高，可以实现宏量制备；纳米管内管径分布很窄，约为20nm；纳米管结构独特，十二胺内嵌入管壁层间成为支撑管子的骨架，并影响管壁层间距；水热反应时间显著影响氧化钒纳米管的生长，理想的水热反应时间为6～8天，因此纳米管热稳定性差。     

多孔钛表面TiO2纳米管的阳极氧化制备及光催化性能（英文）

对多孔钛表面制备TiO2纳米管的阳极氧化工艺进行研究。在两种电解质溶液中采用阳极氧化法分别对多孔钛和钛箔进行表面处理。一种电解质溶液是含有0.5%HF的冰醋酸,另一种电解质溶液是含有0.5%NH4F(质量分数)的乙二醇溶液(醇水体积比4:1)。结果表明:两种方法在钛箔上都可以生成TiO2纳米管,而多孔钛表面只能在NH4F电解质溶液中生成纳米管,HF溶液中过高的电流密度是纳米管在多孔钛基体上难以生成的主要原因。采用扫描电子显微镜和X射线衍射仪对不同基体上的TiO2纳米管进行表征,相比钛箔基体上的纳米管管壁,多孔钛上的纳米管管壁更薄。对所制备的TiO2热处理研究表明,锐钛矿相在400°C时形成,并在700°C完全转变为金红石相。经450°C热处理样品的光催化性能最好。光催化性能也受到多孔钛孔隙率的影响,在孔隙率为60%时光催化性能最好。     

Synthesis and characterization of SrCe0.95Y0.05O3-δ nano powders by low temperature combustion

Nanosized SrCe0.95Y0.05O3-δ powders with homogeneous composition were synthesized by the low temperature combustion process based on the Pechini method. A polymeric precursor sol was formed by using citric acid and ethylene glycol as the chelating agents of metal ions. The perovskite-type SrCe0.95Y0.05O3-δpowders with uniform shape and smaller than 25 nm in size were obtained through the combustion of the polymeric precursor sol at the existence of nitric acid and ammonium hydroxide. It was found that modulating the quantities of nitric acid and ammonium hydroxide could control the particle size, and the quantities of residue carbonate ions were also affected by the quantities of citric acid and ethylene glycol.     

纳米γ-Al2O3的溶胶-凝胶法制备及表征

异丙醇铝为先驱体,异丙醇为溶剂,乙酰乙酸乙酯为螯合剂,聚乙二醇(PEG1000)为分散剂,硝酸为胶溶剂,采用溶胶-凝胶法制备了纳米γ-Al2O3.并采用DTA/TG,XRD,TEM等测试技术对纳米γ-Al2O3粉体进行表征.结果表明,通过溶剂、螯合剂、分散剂和胶溶剂的协同效应,在750℃煅烧条件下,γ-Al2O3粒子形貌为针状结构,长度为20～30 nm;在900℃煅烧条件下,γ-Al2O3粒子形貌为颗粒状,平均晶粒尺寸为10 nm左右;纳米γ-Al2O3粒子尺寸均一、分散性良好.     

柠檬酸法制备热障涂层用La2Ce2O7粉体

以ZrO(NO3)2·2H2O、Ce(NO3)·6H2O和La2O3为原料,采用柠檬酸法制备了La2Ce2O7粉体,研究了pH值、乙二醇及柠檬酸用量、煅烧温度等工艺参数对La2Ce2O7粉体的影响。结果表明,采用该方法能够制备纯净的La2Ce2O7粉体,最佳实验条件是pH值为5,乙二醇、柠檬酸与金属离子的摩尔比分别是1.8和2,煅烧温度为400℃。     

Ni/Ti(C,N)包覆粉及其金属陶瓷的制备

采用非均相沉淀-热还原法制备Ni/Ti(C,N)包覆粉,并用该包覆粉经真空烧结制得金属陶瓷。利用扫描电镜、电子能谱、X-射线衍射等手段研究包覆粉的结构形貌及烧结后的微观组织与性能。结果表明:非均相沉淀过程中,非晶态的NiCO3·2Ni(OH)2·2H2O在Ti(C,N)颗粒表面成核并生长;经热还原过程后,NiCO3·2Ni(OH)2·2H2O分解并完全还原成Ni,Ni的平均晶粒尺寸约为50nm;采用包覆粉为原料制备金属陶瓷,有效改善了硬质相和粘结相的分布均匀性,但包覆粉烧结过程中存在晶粒长大现象;金属陶瓷的相成分为纯净的Ti(C,N)与Ni两相;金属陶瓷的综合性能相对于传统工艺制得的金属陶瓷有一定提高。     

Synthesis and high-temperature performance of Ti substituted α-Ni (OH) 2

Ti substituted α-Ni(OH)2 (c=2.121 nm, a =0. 307 nm) with perfect high-temperature performance was prepared by the co-precipitation method. The effects of Ti addition on the structure and the electrochemical properties were investigated. The results indicate that the substitution of Ti for Ni leads to the conversion of β-Ni(OH)2 to α-Ni(OH)2 and the increase of the inter layer distance along c-axis from 0. 464 nm to 0. 707 nm. Infrared study reveals that more anions(SO2-4 and CO2-3 ions) and H2O exist in the Ti substituted α-Ni(OH)2. The discharge capaciinhibition of the oxygen evolution at high temperature.     

Sol-gel synthesis of Bi3.25La0.75Ti3O12 nanotubes

Ferroelectric Bi_3.25La_0.75Ti₃O₁₂ (BLT) nanotubes were synthesized by sol-gel technique using nanochannel porous anodic aluminum oxide (AAO) templates, and were characterized by X-ray diffraction (XRD), field emission scanning electron microscopy (FE-SEM), transmission electron microscopy (TEM) and high resolution transmission electron microscopy (HRTEM). BLT nanotubes with diameter of around 240 nm and the wall thickness of about 25 nm exhibited a single orthorhombic perovskite structure and highly preferential crystal growth along the [1 1 7] orientation, which have smooth wall morphologies and well-defined diameters corresponding to the diameter of the applied template. The formation mechanism of BLT nanotubes was discussed.     

Erosion–corrosion behavior of aluminum in a 50°C ethylene glycol aqueous solution simulating cooling water in HVDC transmission

The erosion–corrosion of aluminum in a 50 °C ethylene glycol aqueous solution (EGAS) was studied. Compared with that in deionized water, the corrosion of aluminum in an EGAS was inhibited to a certain extent. The corrosion potential, corrosion current, and charge transfer impedance of aluminum changed from −1.5776 V, 380.4 nA cm⁻², and 1.924 × 10⁻⁴ Ω cm⁻² in deionized water to −1.3127 V, 285.5 nA cm⁻², and 4.041 × 10⁻⁴ Ω cm⁻² in a 45.3 vt% EGAS, respectively. Ethylene glycol did not ionize in deionized water and the ionic conductivity of the EGAS was low, effectively restraining the corrosion of aluminum. However, a test with aluminum in an EGAS after long-term storage (9 days) showed that ethylene glycol gradually oxidized to glycolic acid, oxalic acid, and other substances, which slowly corroded the aluminum surface. Analysis results showed that the corrosion products on the surface of aluminum were Al(OH)₃ and Al₂O₃. The pitting hole formation mechanism of aluminum occurs via an aluminum–alcohol phase formed on the aluminum surface, which can inhibit the dissolution of the oxide film. Therefore, a suitably concentrated EGAS with a high heat capacity and low ionic conductivity similar to that of deionized water can be used as a coolant in airtight valve cooling systems for high-voltage direct-current transmission.     

掺钽钨青铜(Ta_xWO_3)的水热合成及电催化性能

以TaCl5和Na2WO4×2H2O为原料,采用水热法在170℃制备性能良好的掺钽钨青铜。并利用XRD、TEM、SEM、UV-vis、IR等谱等分析检测手段对样品的结构和形貌等进行表征,同时研究了掺钽钨青铜的电催化还原氢的性能。结果表明:在170℃合成六方相的掺钽钨青铜,尺寸为10~50 nm。电催化还原氢的实验显示,掺钽钨青铜对氢具有很强的电催化还原活性。     

Fabrication and characterization of anodic oxide nanotubes on TiNb alloys

Titanium and its alloys have been extensively used as implant materials owing to their high specific strength, good biocompatibility and excellent corrosion resistance. Oxide nanotubular array layer can be formed on Ti alloy surface by electrochemical anodization treatment. In this work, the morphology of nanotubes formed on Ti–Nb alloys(Nb content of 5 wt%, 10 wt%, 20 wt%, 30 wt% and40 wt%) was investigated using an electrolyte containing ethylene glycol and NH_4 F. Oxide layers consisting of highly ordered nanotubes with a range of diameters(approximately40–55 nm for the inner diameter and 100–120 nm for the outer diameter) and lengths(approximately 10–20 lm) can be formed on alloys in the Ti–x Nb system, independent on the Nb content. The nanotubes formed on the Ti–Nb alloy surface were transformed from the anatase to rutile structure of titanium oxide. The oxide nanotubular surface is highly hydrophilic compared with the intact Ti Nb foil. The surface wettability varies with the nanotube diameter. As the nanotube diameter increases while the nanotube layer thickness remains constant, the capillary wetting of the nanotube surface decreases and the surface becomes less hydrophilic.Annealing changes the nanotubular surface wettability further and establishes less hydrophilic surface conditions due to the removal of hydroxyl groups and residue fluoridecontaining species. It is believed that the surface wettability is changed due to the decreasing content of hydroxyl groups in ambient atmosphere. This work can provide guidelines for improving structural and environmental conditions responsible for changing surface wettability of Ti Nb surfaces for biomedical applications.